EP0968258B1 - Verfahren und vorrichtung zum reinigen von verunreinigungen enthaltenden flüssigkeiten - Google Patents

Verfahren und vorrichtung zum reinigen von verunreinigungen enthaltenden flüssigkeiten Download PDF

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Publication number
EP0968258B1
EP0968258B1 EP98916994A EP98916994A EP0968258B1 EP 0968258 B1 EP0968258 B1 EP 0968258B1 EP 98916994 A EP98916994 A EP 98916994A EP 98916994 A EP98916994 A EP 98916994A EP 0968258 B1 EP0968258 B1 EP 0968258B1
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EP
European Patent Office
Prior art keywords
liquid
particles
adsorbent
agglomerator
outlet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP98916994A
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German (de)
English (en)
French (fr)
Other versions
EP0968258A1 (de
Inventor
Peter Transfeld
Gunter BÖRNER
Matthias Schneider
Rainer Wetzel
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
OEHMI AKTIENGESELLSCHAFT
Original Assignee
Ohmi AG
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Publication date
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Publication of EP0968258A1 publication Critical patent/EP0968258A1/de
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Publication of EP0968258B1 publication Critical patent/EP0968258B1/de
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
    • C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
    • C10G53/08—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one sorption step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • C11B3/10—Refining fats or fatty oils by adsorption

Definitions

  • the invention relates to a method for cleaning contaminants Liquids, with the addition of adsorbents, and a Device for performing this method.
  • DE 43 44 828 A1 describes a method and a device known for cleaning liquids containing impurities, at which the contaminated liquid by means of mutually insulated electrodes electrical field is exposed, while the viscosity of the cleaning liquid is reduced by heating. With this procedure part of the liquid can be removed after cleaning, but remains a not inconsiderable part of the liquid in the cloudy run. It is also disadvantageous that the design and control of the electrodes is complex.
  • the invention has for its object a method and an apparatus for cleaning liquids containing impurities, such as oils and Specify bold, where the separation with little equipment and energy consumption takes place.
  • the relatively fine-grained adsorbent particles adsorb Impurities in the liquid as solid particles or dye or are otherwise present and should be removed. After or during that Adsorbent particles that have taken up impurities will now become one Agglomeration of the fine-grained adsorbent particles made.
  • the suspension is first an electrical one for a certain time Field exposed, with the charged particles moving to an electrode become.
  • These particles agglomerate there, are separated and when switched off of the electric field resuspended in the liquid, the Adsorbent particles through the agglomeration an enlarged particle structure exhibit.
  • the particles have a porous, loose structure.
  • the subsequent filtration which is preferably carried out as pressure filtration, is can be carried out more effectively because of the enlarged particle structure, since the enlarged ones Particles in the formation of the filter cake sufficient permeability allow for the liquid. According to the invention, it is thus possible to operate the filtration up to a considerably higher loading of the filter surface.
  • the invention becomes particularly effective if it is used as a sub-step in one Countercurrent bleaching method is used, as it is for example in the post-published German patent application 196 20 695.2-41 is described.
  • Countercurrent processes unpurified oils are added in one step already partially loaded adsorbent in contact and then in one second stage, the oil partially cleaned in the first stage with fresh adsorbent.
  • the adsorbent used in this second stage then serves in the first Stage as a partially loaded adsorbent. Bottom line of the second stage is then highly purified oil.
  • the concentrated suspension now created according to the invention with the Already agglomerated and loaded adsorbent particles can be used in such Counterflow process now treated as the "partially loaded adsorbent" and introduced in the first stage together with the still unpurified oil become.
  • the agglomerated adsorbent particles can again save resources be used.
  • the bleaching earth to be supplied has a large proportion of fine grains, for example, with a grain spectrum of 5 to 10 microns, is due to the enlarged free surface of the fine-grained bleaching earth the adsorption power elevated. It is therefore no longer necessary to meter excess bleaching earth.
  • the bleaching earth consumption is thus advantageously reduced.
  • the use of bleaching earth can, for example, with rapeseed oil from the usual minimum of 0.6% to 0.3% be absolutely reduced.
  • the fine-grained bleaching earth is in the Procurement costs cheaper than the previously used, through pretreatment structured bleaching earth. So far, the grain size distribution has been a problem Compromise between a sufficiently good bleaching effect and a sufficient one good separability through conventional filter systems. Since according to the invention but started with fine-grained bleaching earth with high adsorption power is and this is aggregated into coarser particles, is the The suspension is optimally structured for the subsequent filtration.
  • a particularly economical pressure filtration is achieved if the solids content the concentrated suspension to 10% to 30%, preferably 17% to 20%.
  • the process according to the invention is preferably operated batchwise, initially a batch of liquid to be cleaned is an electrical Field exposed and agglomerated, possibly a fraction of purified liquid is subtracted, the electrical field is subsequently switched off and the Suspend adsorbent particles in the (remaining) liquid, after which the concentrated Suspension is filtered.
  • pressure filtration can also be economical be carried out, in particular when reaching a certain Filter cake load the pressure filtration can be interrupted at any time, to discharge the filter cake.
  • these units can feed the pressure filtration with a time delay the entire process runs continuously despite the batchwise agglomeration.
  • a partial stream of solid particles Liquid of the agglomeration and the subsequent renewed suspension is suspended, the concentrated suspension not processed other partial flow of the liquid fed and filtered together becomes.
  • the enlarged ones contained in the concentrated suspension Particle structures increase the permeability in the subsequent pressure filtration of the filter cake building up. This means that partial treatment is also possible more economical cleaning can be achieved.
  • the object is achieved in that at least one agglomerator with an inlet, one outlet each for the separate components (Clear run, concentrated suspension) and a device for production agglomeration, in particular an electric field, and a pressure filter with an inlet for the concentrated suspension and one outlet for each the separate components (clear run, filter cake) are provided.
  • the liquid to be cleaned is in the agglomerator with the device for Generation of an electric field, for example on an electrode side, collected and agglomerated.
  • the top Already cleaned liquid.
  • the agglomerated particles are again in the residual liquid suspended and via the second outlet as a concentrated suspension fed to the pressure filter. From there, an outlet delivers the cleaned liquid out. If necessary, the second outlet of the pressure filter can be used Filter cakes are removed.
  • a first collecting container in the inlet before the agglomerator is provided to a in batch operation of the agglomerator to enable independent liquid supply.
  • a vacuum pump is connected to the first reservoir, can a low pressure of, for example, 40 to 120 mbar can be set.
  • the liquid in the container heat to a temperature of 90 ° C to 130 ° C.
  • a second collection container is provided at the outlet of the agglomerator whose outlet leads to the pressure filter via a pump can be cleaned the supply of concentrated suspension is briefly interrupted by the pressure filter without disturbing the operation of the agglomerator.
  • the concentrated suspension is buffered in the second collection container.
  • FIG. 1 schematically shows the structure of a device for cleaning liquids containing impurities in a first embodiment.
  • An inlet for the suspension to be cleaned is indicated by an arrow 1.
  • the feed line leads via a feed pump 4 to four agglomerators 10, 10 ', 10 ", 10"' connected in parallel.
  • the agglomerators are designed to match and are operated alternately.
  • the agglomerator 10 has an inlet opening 11 to which the inlet 1 of the suspension to be cleaned which is fed via the inlet pump 4 is connected.
  • a device 12 for generating an electric field which can be constructed, for example, from two electrodes or electrode systems.
  • each of the agglomerators 10, 10 ', 10 ", 10"' there is an outlet 13 for the component of the liquid which has already been cleaned in the agglomerator, the clear run.
  • This outlet 13 is located in the upper part of the agglomerator to prevent contaminants from getting into the clear run.
  • At the lower end of each agglomerator 10, 10 ', 10 ", 10"" there is an outlet 14 for the concentrated suspension.
  • the outlet 14 of each agglomerator 10, 10', 10", 10 "' is combined and via a valve 21 connected to a second collecting container 20.
  • the agglomerate or concentrate is thus in the collecting container 20 or the concentrated suspension.
  • An outlet line 22 leads from the second collecting container 20 for the concentrated one Suspension to an inlet 31 of a pressure filter 30.
  • a valve 35 and a slurry pump 36 are arranged in this connecting line.
  • the Mud pump 36 presses the concentrated suspension against the Pressure filter 30 arranged precoat filter 32 to a filter cake there form.
  • the liquid passing through the filter 32 is through an outlet 33 of the pressure filter 30 led to a drain line indicated by arrow 2, to which the outlets 13 of the agglomerators 10, 10 ', 10 ", 10"' are also connected are.
  • the filtrate thus leaves the drain line indicated by arrow 2 Cleaning process.
  • an outlet 34 is arranged, which over a Valve 37 to an outlet 3 marked with an arrow for the discharge to be carried out pasty mass (filter cake) leads.
  • a bleaching stage 40 to 47 is connected upstream of the inlet 1.
  • the bleaching stage consists of a first collecting container 40 which has an inlet 41 for filling with the liquid to be cleaned and a further inlet 48 for the fresh adsorbents.
  • a suction opening 42 with a valve 43 and a vacuum pump 44 for generating a negative pressure in the container is arranged on the first collecting container 40.
  • a line indicated by arrow 47 schematically shows the vacuum here.
  • an outlet 45 with a valve 46 for discharging the liquid loaded with the adsorbents.
  • This liquid is fed to an inlet 11 of an agglomerator 10 via the inlet pump 4.
  • a single agglomerator 10 is provided, so that this device can be operated in batches.
  • the agglomerator 10 there is an electrode arrangement 12 for generating a electrical field arranged.
  • the clear run of the agglomerator is controlled by a arranged in the upper part of the container outlet 13 to an inlet 51 a third collecting container 50 out.
  • an outlet 14 At the bottom of the agglomerator 10 is an outlet 14 with a valve 21 for the concentrated suspension intended.
  • An outlet 22 of the second collection container 20 leads via inlet 35 and sludge pump 36 to an inlet 31 Pressure filter 30.
  • the pressure filter 30 has a precoat filter construction 32 on the inside, which Collect suspended particles of the concentrated suspension.
  • the pressure filter 30 has an outlet 33 for the filtrate, which is connected to an inlet 52 of the third Container 50 is connected. Furthermore, the pressure filter 30 has at its lowest End of a drain opening 34 with valve 35 for discharging the filter cake according to arrow 3.
  • the third collecting container 50 contains the cleaned liquid. At its bottom At the end is an outlet 53 with a valve 54 for dispensing the cleaned liquid provided according to arrow 2.
  • the liquid contaminated with impurities is supplied essentially continuously to at least one agglomerator 10, 10 ', 10 ", 10"' via the feed pump 4.
  • the agglomerators are filled in batches one after the other in stages.
  • the second agglomerator 10 ' is then filled with the suspension to be cleaned, while in the first agglomerator 10 the liquid is exposed to an electric field by means of the electrodes 12.
  • the solid particles are collected on one side of the electrode and agglomerated. On the other side, there is then cleaned liquid which is fed to the clear run via outlet 13.
  • the third agglomerator 10 "is already filled with the suspension to be cleaned, while in the second agglomerator 10 'the liquid is already exposed to an electrical field.
  • the electrical field in the first agglomerator 10 has been switched off, the solid particles accumulated on the electrode suspend in the remaining liquid, thus creating a concentrated suspension.
  • the fourth agglomerator 10 '" is already being filled with the suspension to be cleaned, the concentrated suspension is withdrawn from the first agglomerator 10 via outlet 14.
  • the first agglomerator 10 is now ready to take up the next batch of liquid to be cleaned.
  • the concentrated suspension is temporarily stored in a second collecting container 20 and by means of valve 35 and slurry pump 36 if necessary fed to the pressure filter 30.
  • the valve 35 is open and the pump 36 is operated until the precoat filters arranged in the pressure filter 30 32 filter cakes formed has reached a maximum strength.
  • valve 35 is closed and the filter cake built up on the precoat filters via outlet 34 and Valve 37 discharged as a pasty mass.
  • the process sequence according to the embodiment according to FIG. 2 is similar in principle , only one agglomerator 10 being provided, so that the system is to be operated in batches.
  • the liquid to be cleaned is supplied with 48 adsorbents via the inlet, which are heated in a first reservoir 40 and kept at reduced pressure.
  • the adsorbents supplied adsorb the impurities contained in the liquid in this container.
  • the liquid loaded with the adsorbents is now fed to the cleaning process already described.
  • the particles in the liquid, in particular the adsorbents, as low as possible in the adsorption stage Particle size have an optimal adsorption effect with low consumption of adsorbents.
  • the one there resulting, concentrated suspension is due to the increased particle size optimally pre-structured for pressure filtration.
  • the bleached oil is pumped as a suspension into the agglomerator 10, which has a separation area of 0.4 m 2 as the electrode.
  • a voltage of 20 kV is applied to the electrodes while the agglomerator is being filled.
  • the voltage is then increased to 30 to 40 kV.
  • the bleaching earth contained in the suspension and loaded with impurities now moves to the positive electrode, the separation surface, and agglomerates in the process.
  • the clear oil emerging above the positive electrode at the outlet 13 is in the third collection container 50 collected. After a certain time, approx. 15 min, the capacity of the separation area is exhausted and the feed pump is turned off. After switching off the electrical field, the on suspend the positive electrode agglomerated bleaching earth particles again in the oil. The content of the agglomerator is now led into the sludge tank 20. The oil and the agglomerated bleaching earth gives a suspension with 10% to 30% Bleaching earth for the subsequent pressure filtration. This procedure described is now repeated until about 100 l of concentrated suspension (Mud) are present.
  • This concentrated suspension is then moved by means of the sludge pump 36 over a modified precoat filter with a filter area of 0.2 m 2 .
  • This filtration is operated up to a load of 85 kg per m 2 of filter area.
  • the rest of the clear oil is also collected in the collecting container 50, while the filter cake is discharged downwards as a pasty mass.
  • the usual drying by blowing out with compressed air or steam to a residual oil content of 20 to 30% is possible below.
  • the procedure according to the invention thus allows adsorbents of any structure, For example, use bleaching earth with maximum fine grain content.
  • FIG. 3 represents a countercurrent bleaching method based on the otherwise published German patent application 196 20 695.2-41.
  • the reference numerals here are arranged on functionally similar elements as in the two other exemplary embodiments discussed above. However, the process is sometimes somewhat different.
  • the suspension to be cleaned is fed into a container 20.
  • This container 20 is connected via a line 14 to the outlet Sludge from another stage, namely the agglomerator 10, which is described further below.
  • From the collection container 20 is about a pump 36 the resulting total or mixture of partially cleaned Suspension with the sludge and the heavily soiled contained therein Bleaching earth portion fed two pressure filters 30.
  • the outlet 33 from the pressure filter 30 leads the rest, so the now partially cleaned suspension, to another container, by supplementing it with fresh bleaching earth from an inlet 48 and the first Collection container 40 is supplied, which contains a mixer here.
  • This Mixer 40 mixes the already cleaned and only relatively little dirt containing liquid or suspension with the over strong cleaning power, namely fresh bleaching earth.
  • This Mixture is now fed to the agglomerator 10 via the pump 4, the above has already been mentioned.
  • the agglomerator 10 now operates similarly to that in the first Described embodiments, so that reference is made here.
  • the agglomerator 10 can additionally work as it does in the German one Patent application 196 20 695.2-41 is described. On the content as far as expressly referred.
  • the collection containers 20 and 40 and the intermediate container are in turn a line 47 connected to vacuum.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Wood Science & Technology (AREA)
  • Analytical Chemistry (AREA)
  • Electrostatic Separation (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
EP98916994A 1997-03-18 1998-03-18 Verfahren und vorrichtung zum reinigen von verunreinigungen enthaltenden flüssigkeiten Expired - Lifetime EP0968258B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19711174 1997-03-18
DE19711174A DE19711174A1 (de) 1997-03-18 1997-03-18 Verfahren und Vorrichtung zum Reinigen von Verunreinigungen enthaltenden Flüssigkeiten
PCT/EP1998/001567 WO1998041596A1 (de) 1997-03-18 1998-03-18 Verfahren und vorrichtung zum reinigen von verunreinigungen enthaltenden flüssigkeiten

Publications (2)

Publication Number Publication Date
EP0968258A1 EP0968258A1 (de) 2000-01-05
EP0968258B1 true EP0968258B1 (de) 2001-12-05

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EP98916994A Expired - Lifetime EP0968258B1 (de) 1997-03-18 1998-03-18 Verfahren und vorrichtung zum reinigen von verunreinigungen enthaltenden flüssigkeiten

Country Status (12)

Country Link
US (1) US6656364B1 (zh)
EP (1) EP0968258B1 (zh)
JP (1) JP2001517142A (zh)
CN (1) CN1140614C (zh)
AR (1) AR010131A1 (zh)
AU (1) AU7036898A (zh)
BR (1) BR9808921A (zh)
CA (1) CA2279365A1 (zh)
DE (2) DE19711174A1 (zh)
MY (1) MY122118A (zh)
TR (1) TR199902006T2 (zh)
WO (1) WO1998041596A1 (zh)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CL2007002515A1 (es) * 2006-09-01 2008-03-14 Grace Gmbh & Co Kg Metodo de procesamiento de un fluido usando un sistema de filtracion escalonada que comprende pasar fluido a traves de dos o mas filtros de pre-blanqueo, filtrar el fluido a traves de uno o mas filtros de post-blanqueo; y aparato adecuado para proces
TWI392538B (zh) * 2010-05-19 2013-04-11 Univ Nat Sun Yat Sen 具有電極之濾板組及使用該濾板組之壓濾機
CN104474746A (zh) * 2014-11-17 2015-04-01 江西麻山化工有限公司 一种悬浮液中微粒子沉降方法
CN109337711B (zh) * 2018-12-03 2020-11-06 河北科技师范学院 一种液压油循环净化设备
US11977166B2 (en) * 2019-08-16 2024-05-07 WeRide Corp. Optical system, method and apparatus for diagnosing the same
CN112266161B (zh) * 2020-10-30 2023-04-14 烽火通信科技股份有限公司 一种用于d4液体原材料的汽化装置及方法

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2618644A (en) * 1948-11-04 1952-11-18 Girdler Corp Method for bleaching oil with adsorbent
US2717256A (en) 1951-08-28 1955-09-06 Nat Cylinder Gas Co Oil bleaching method
US3763040A (en) 1971-08-13 1973-10-02 Environmental Protection Agenc Processes for reducing the organic-carbon content of water contaminated with organic compounds by continuous countercurrent multistage treatment with activated carbon
FI51905C (fi) 1974-06-20 1977-05-10 Neste Oy Menetelmä ja laite nesteen adsorptiosuodattamiseksi.
US4040926A (en) * 1975-11-28 1977-08-09 Petrolite Corporation Electrofiltration process for purifying organic liquids
US4049520A (en) * 1976-03-19 1977-09-20 Petrolite Corporation Color improvement process for organic liquid
DE4124331C2 (de) 1991-07-23 1993-11-25 Oehmi Forsch & Ingtech Gmbh Verfahren und Vorrichtung zur adsorptiven Reinigung von pflanzlichen und/oder mineralischen Ölen und Fetten
DE4210795C1 (en) * 1992-04-01 1993-05-06 Oehmi Forschung Und Ingenieurtechnik Gmbh, O-3060 Magdeburg, De Adsorptive purificn. of vegetable and/or mineral oils and fats - in multistage counterflow, with fresh adsorbent and pre-purified oil introduced into first mixer
DE4344828A1 (de) * 1993-12-28 1995-06-29 Oehmi Forsch & Ingtech Gmbh Verfahren und Vorrichtung zum Reinigen von Feststoffpartikeln enthaltenden Flüssigkeiten
DE19620695C1 (de) * 1996-05-23 1997-05-15 Oehmi Forsch & Ingtech Gmbh Verfahren und Vorrichtung zur adsorptiven Reinigung von pflanzlichen und/oder mineralischen Ölen und Fetten

Also Published As

Publication number Publication date
AR010131A1 (es) 2000-05-17
WO1998041596A1 (de) 1998-09-24
DE19711174A1 (de) 1998-09-24
DE59802335D1 (de) 2002-01-17
JP2001517142A (ja) 2001-10-02
CN1250467A (zh) 2000-04-12
TR199902006T2 (xx) 2000-04-21
AU7036898A (en) 1998-10-12
US6656364B1 (en) 2003-12-02
MY122118A (en) 2006-03-31
CA2279365A1 (en) 1998-09-24
CN1140614C (zh) 2004-03-03
EP0968258A1 (de) 2000-01-05
BR9808921A (pt) 2000-08-01

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